WO2008086525A2 - Systèmes à haut rendement pour résonance magnétique nucléaire avec rotation à l'angle magique - Google Patents

Systèmes à haut rendement pour résonance magnétique nucléaire avec rotation à l'angle magique Download PDF

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Publication number
WO2008086525A2
WO2008086525A2 PCT/US2008/050905 US2008050905W WO2008086525A2 WO 2008086525 A2 WO2008086525 A2 WO 2008086525A2 US 2008050905 W US2008050905 W US 2008050905W WO 2008086525 A2 WO2008086525 A2 WO 2008086525A2
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WIPO (PCT)
Prior art keywords
probe
angle spinning
magic angle
modules
solid
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PCT/US2008/050905
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English (en)
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WO2008086525A3 (fr
Inventor
Eric J. Munson
Dewey H. Barich
Benjamin N. Nelson
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University Of Kansas
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Publication of WO2008086525A2 publication Critical patent/WO2008086525A2/fr
Publication of WO2008086525A3 publication Critical patent/WO2008086525A3/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
    • G01R33/307—Sample handling arrangements, e.g. sample cells, spinning mechanisms specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/42—Screening
    • G01R33/422—Screening of the radio frequency field

Definitions

  • This invention relates to a magic angle spinning (“MAS”) nuclear magnetic resonance (“NMR”) probe for the analysis of solids and semi-solids.
  • MAS magic angle spinning
  • NMR nuclear magnetic resonance
  • the invention relates to a probe having two or more MAS systems within the homogeneous region of the magnetic field.
  • Solid-state NMR spectroscopy is a powerful technique for the analysis of solids and semi-solids. It is a non-destructive and non-invasive technique that can provide selective, quantitative, and structural information about the sample being analyzed.
  • New drug compounds often are poorly crystalline or even amorphous, have long relaxation times, and are present at low levels in a formulation. This creates a significant problem for analyzing these compounds using solid-state NMR spectroscopy, because analysis times can range from a few minutes to a few days depending upon the state of the sample (i.e., bulk drug or formulated product), relative sensitivity (i.e., choice and number of different nuclei in molecule), and relaxation parameters.
  • aspirin is a representative pharmaceutical solid, and has a Ti relaxation time of approximately 30 seconds at 300 MHz such that the pulse delay between acquisitions must be at least 90 seconds to avoid saturation. With salicylic acid, the delay between acquisitions exceeds one hour.
  • Patent No. 6,696,838 Raftery showed that up to four different non-spinning samples could be located simultaneously in the homogeneous part of the magnetic field. The more non-spinning samples, however, the smaller the sample volume must be for all samples to be located simultaneously in the homogeneous region of the magnetic field.
  • the present invention is directed to a novel solid-state nuclear magnetic resonance probe for use in a magnetic field comprising: a housing adapted to be placed in the magnetic field; and a plurality of isolated magic angle spinning modules positioned within the housing, the isolated spinning modules being configured to hold different samples for solid-state NMR analysis.
  • the housing is configured so that the plurality of magic angle spinning modules are located within a homogeneous region of the magnetic field.
  • the modules may be placed as close together as possible, typically less than 3 cm apart as measured from the center of one coil to the center of the other coil in the MAS modules.
  • the probe further comprising a radio-frequency isolation shield configured to reduce cross talk between said magic angle spinning modules.
  • the samples may be the same or different material for analysis.
  • the invention is directed to a solid-state nuclear magnetic resonance spectrometer comprising: a magnet, the magnet defining a bore; a probe having at least two magic angle spinning modules; and an acquisition device coupled to the magic angle spinning modules, the acquisition device being configured to acquire a signal from said isolated spinning modules.
  • the probe is configured so that at least two magic angle spinning modules are located within a homogeneous region of the magnetic field.
  • the present invention is directed to a method for the analysis of a solid-state sample comprising the steps of: providing a magnet for generating a magnetic field, the magnet defining a bore; providing a probe having a first isolated magic angle spinning module and a second isolated magic angle spinning module; positioning the probe within the bore of the magnet so that the first and second magic angle spinning modules are within a homogeneous region of said magnetic field; acquiring a first spectrum from a first sample contained within the first magic angle spinning module; and acquiring a second spectrum from a second sample contained within the second magic angle spinning module.
  • the step of acquiring the first spectrum and the step of acquiring the second spectrum may be performed simultaneously or sequentially.
  • FIG. 1 is a schematic view of an embodiment of a solid-sate NMR probe having two MAS modules in accordance with the present invention.
  • the MAS modules are spaced so that both may be statically positioned within the homogeneous region of the magnetic field.
  • FIG. 2 illustrates a solid-state NMR probe that contains two MAS modules located in the homogeneous region of the magnet.
  • FIG. 3 is a plot of line width vs. distance from the homogeneous region of the magnet.
  • samples such as adamantane and 3-methylglutaric acid (“MGA”)
  • MCA 3-methylglutaric acid
  • narrow lines can be obtained in a range of 0 to 1 cm from the original location of the probe.
  • lines with somewhat broader peaks there may not be a significant change in line width up to 1.25 cm from the original location of the probe.
  • the graph may not be symmetric, i.e., the negative position values were not measured.
  • Hexamethylbenzene HMB was used as a standard.
  • the present invention relates to solid-state NMR spectroscopy.
  • the present invention is directed to the use of a probe that increases sensitivity and throughput of samples being analyzed with solid-state NMR.
  • a magic-angle spinning ("MAS") NMR probe is described to increase sensitivity and throughput, the probe including multiple spinning systems within the homogeneous region of a static magnetic field of a superconducting magnet.
  • solid-state and sample refer to any material, compound, or sample that is a solid or semi-solid.
  • sample refer to any material, compound, or sample that is a solid or semi-solid.
  • “different samples” means samples contained within different MAS modules. The material being analyzed that is contained within the "different samples” may be the same or different.
  • plural means more than one.
  • coupled means a direct or indirect connection between two or more elements.
  • the term "homogeneous region" of the magnetic field refers to the region in the magnetic field in which, under MAS conditions, the line width as defined by full width at half height of a sample (such as adamantane) is below a threshold value of about 0.5 ppm, and preferably below about 0.3 ppm, and most preferably below about 0.1 ppm.
  • the NMR probe 10 includes two magic-angle spinning ("MAS") systems or modules 20, 40.
  • MAS magic-angle spinning
  • the number of modules can be increased, but is typically two, three, or four MAS modules.
  • the preferred MAS modules may be obtained from Revolution NMR (Fort Collins, CO). Any suitable MAS module can be utilized.
  • the probe 10 can be constructed to use typical MAS modules (for example, 4 or 7 mm o.d. rotors).
  • the probe 10 includes a framework or housing 60 that houses the MAS spinning systems or modules 20, 40.
  • a shield (not shown) can be placed around the housing 60 to protect the components of the probe 10.
  • the MAS modules 20, 40 are attached to mounting plates 16, 17 at attachment points 21, 22 for the first module 20 and attachment points 41, 42 for the second module 40. Between the two MAS modules 20, 40 is a radio frequency ("RF") isolation shield 55.
  • RF radio frequency
  • the first MAS module 20 is coupled to a fixed capacitor 23 (American Technical Ceramics, Huntington Station, NY) for the tuning of the first MAS module 20.
  • the fixed capacitor 23 roughly tunes (+/- 3 MHz) the RF circuit for this first MAS module 20.
  • MAS module 20 is coupled to RF transmission line 25.
  • the RF transmission line 25 can be a coaxial cable.
  • the system for tuning the first module 20 is preferably compact so that additional modules can be positioned no further than 3 cm apart.
  • the MAS modules 20, 40 in the probe 10 are about 2.1 cm apart if both of the MAS modules 20, 40 are designed to use 7 mm o.d. rotors.
  • the MAS modules 20, 40 can be positioned closer together if one or both are designed to use smaller rotors (presently, MAS modules are available commercially with rotors as small as 2 mm o.d.).
  • a second portion of the tuning circuit can be located outside the probe. This tuning circuit can be designed for fixed frequencies with fine-tuning of the circuit performed below the magnet.
  • Gas is provided to first module 20 through supply lines 27, 28 for the spinning and stabilization of a first sample holder positioned within the first MAS module 20.
  • supply lines 27, 28 for the spinning and stabilization of a first sample holder positioned within the first MAS module 20.
  • the ability to supply sufficient spinning/bearing air to each module is not trivial. Individual air lines are provided for each MAS module, although space considerations may require alternative air supply methods.
  • the first sample holder is a compact spinning MAS device (Revolution NMR, Fort Collins, CO).
  • Supply lines 27, 28 provide gas (preferably air) in order to rotate the first sample holder positioned within sample cavity 29 defined by the first MAS module 20 and for bearing of the first sample holder within the first module 20, respectively.
  • a first MAS adjustment device 30 can be coupled to the first MAS module 20 for adjusting the angle of the first MAS module 20 relative to the magnetic field of a superconducting magnet.
  • the first MAS adjustment device 30 can be used to adjust the angle of the first MAS module 20 and the sample contained with the module 20 to maximize the signal obtained during an experiment conducted on the first sample. An angle of 54.7 degrees relative to the magnetic field of the magnet is preferred. While the MAS module 20 is stationary during data acquisition by the spectrometer, it will be appreciated that the position of the MAS module may be adjusted when the spectrometer is not in use.
  • a first rotation measuring device 31 employing means such as fiber optics, can be coupled to the first MAS module 20 for measuring the rotational speed of the first sample holder contained within the first MAS module 20.
  • a distinctive mark can be placed on the first sample holder to facilitate the measurement of the rotational speed of the first sample holder.
  • Computer control software (such as LabView available from National Instruments, Austin, TX) can be used to maintain spinning speed control for the first sample holder contained within the first module 20.
  • the second MAS module 40 is coupled to a fixed capacitor 43 for the tuning of the second MAS module 40.
  • MAS module 40 is coupled to RF transmission line 45.
  • the RF transmission line 45 can be made of coaxial cables.
  • the system for tuning the second module 40 is also preferably compact so that additional modules can be positioned no further than 3 cm apart. Utilizing variable tuning elements in the probe eliminates the need for a mechanism (such as plastic rods) for changing large variable capacitors that tune the circuit for the second module 40. A second portion of the tuning circuit can be located outside the probe. This tuning circuit can be designed for fixed frequencies with fine-tuning of the circuit performed below the magnet.
  • Gas is provided to second MAS module 40 through supply lines 47, 48 for the spinning and stabilization of a second sample holder positioned within the second module 40.
  • the second sample holder is also a compact spinning MAS device (Revolution NMR, Ft. Collins CO).
  • Supply lines 47, 48 provide gas (preferably air) in order to rotate the second sample holder positioned within a second sample cavity 49 defined by the second module 40 and for bearing of the second sample holder within the second module 40, respectively.
  • a second MAS adjustment device 50 can be coupled to the second MAS module 40 for adjusting the angle of the second MAS module 40 relative to the magnetic field of a superconducting magnet.
  • the MAS adjustment device 50 can be used to adjust the angle of the second MAS module 40 and the sample contained with the module 50 to maximize the signal obtained during an experiment conducted on the second sample. An angle of 54.7 degrees relative to the magnetic field of the magnet is preferred. While the MAS module 40 is stationary during data acquisition by the spectrometer, it will be appreciated that the position of the MAS module may be adjusted when the spectrometer is not in use.
  • the MAS modules 20, 40 are illustrated in FIG. 1 as being vertically aligned directly on top of one another, it will be appreciated that the position of the MAS modules 20, 40 may be altered (for example, such that MAS module 20 is not directly above MAS module 40), provided that both MAS modules are positioned in a stationary position within the homogeneous region of the magnetic field during data acquisition.
  • a second rotation measuring device 51 can be coupled to the second MAS module 40 for measuring the rotational speed of the second sample holder contained within the second MAS module 40.
  • a distinctive mark also can be placed on the second sample holder to facilitate the measurement of the rotational speed of the second sample holder.
  • the same computer control software used for the first sample holder can be used to maintain spinning speed control for the second sample holder contained within the second MAS module 40.
  • compact spinning modules such as those commercially available from Revolution NMR (Fort Collins CO) are particularly advantageous.
  • the minimum distance between MAS modules that does not sacrifice RF performance or magnetic field homogeneity can be determined.
  • the MAS modules may be less than about 3 cm, 2.9 cm, 2.8 cm, 2.7 cm. 2.6 cm, 2.5 cm, 2.4 cm, 2.3 cm. 2.2 cm, 2.1 cm, 2.0 cm, 1.9 cm, 1.8 cm, 1.7 cm. 1.6 cm, 1.5 cm, 1.4 cm, 1.3 cm. 1.2 cm, 1.1 cm, or 1.0 cm.
  • each MAS module 20, 40 might have different field homogeneity requirements, requiring separate shim parameters. For example, if the field homogeneity requirements of each MAS module 20, 40 are different, then the shim parameters for each MAS module 20, 40 can be optimized separately and stored. In such a case, one step taken when switching signal acquisition from one of the MAS modules 20, 40 to the other would be to apply the shim parameters associated with the MAS module 20, 40 that is next to undergo data acquisition.
  • the magic angle of the MAS modules 20, 40 can be adjusted at the bottom of the NMR probe 10. This can be done by having individual MAS adjustors extending from the bottom of the probe 10. Preferably, a single MAS adjustor can be used to replace a system that has multiple MAS adjustors extending out of the probe.
  • This MAS adjustor which can be adjusted to reposition both of the modules 20, 40, requires that the probe 10 be lowered out of a magnet for adjustment of the magic angle. Since the probe 10 is designed to be raised and lowered within the magnet, having the probe extend below the magnet would also enhance sample changing.
  • High-power RF switches can be used to direct the output to the individual circuits for the MAS modules 20, 40. Switches are available with power handling capabilities of more than 350 W CW and switching times of less than 20 ms. Alternatively, separate spectrometers can be utilized to control and acquire data from the separate modules 20, 40. Other known techniques for control and acquisition of data from the MAS modules 20, 40 can also be utilized.
  • Utilizing a probe such as probe 10 results in little or no loss in field homogeneity, sensitivity, MAS speed, or 1 H decoupling field strength compared to conventional NMR probes. While this approach can be used at any magnetic field strength, it works better at higher field strengths, where Ti relaxation rates are much longer than at lower field strengths. Higher fields also imply faster spinning systems and therefore smaller sample volumes. However, this means that more spinning systems could be placed in the static magnetic field, enabling more samples to be run.
  • the probe 10 of FIG. 1 is shown positioned within a superconducting magnet 90 as ref no. 110.
  • Probe 110 is inserted into the bore 91 of the magnet 90.
  • Gas lines 47 and 48 are shown coupled to the probe 110.
  • the two MAS module probe 110 shown in FIGS. 1 and 2 is a double-resonance ( 1 H- 13 C) probe, which results in one RF transmission line being coupled to each of the MAS modules 120, 140.
  • the probe shown in FIG. 2 includes two separate coils distanced less than about 3 cm apart, more specifically about 2.1 cm apart as measured from the center of one coil to the center of the other coil. This distance, along with RF isolation shield 55, reduces cross-talk between coils.
  • Probe 110 operates for the analysis of different samples contained within a solid-state NMR probe as follows. Both MAS modules 120, 140 are placed inside the homogeneous region of the magnetic field 150.
  • the device 100 may be used in a mode where simultaneous acquisition of signals from both MAS modules 120, 150 is performed. More specifically, each MAS module 120, 140 is associated with a respective signal acquisition device, and each device is independently controlled.
  • the preferred mode is to acquire the signals from each of the MAS modules 120, 140 located within the homogeneous region of the magnetic field sequentially. That is, because the delay between the end of signal acquisition and the beginning of the next set of acquisition (often referred to as the pulse delay) for most solid or semi-solid samples is at least an order of magnitude greater than the acquisition time, there is sufficient time to switch between samples and acquire the signal sequentially. It may also be practical that if the signal from the first sample is much stronger than from the second sample, then the signal from the second sample should be acquired right after the signal from the first sample. At that time the signal from the first sample will be saturated, and will have a minimal contribution to the signal from the second sample. An alternative would be to saturate the signal from the first sample prior to acquiring the signal from the second sample. This may be feasible if the signal from the first sample had a relatively short relaxation time, and the second sample had a longer relaxation time.
  • a solid-state NMR spectrometer having more than two MAS modules may be constructed. Typically, there will be two, three, or four MAS modules within the homogeneous region of the magnetic field.
  • RF transmission lines are used to connect the probe to a remote RF tuning device and switching box.
  • the RF tuning device and switching box can be separately housed or housed within a single device.
  • This box serves two purposes.
  • each MAS module can be selected independently for signal acquisition.
  • High-power RF switches can be used to direct the output to the individual circuits for the modules. As described above, switches are available with power handling capabilities of greater than 350 W CW and switching times of less than 20 ms. Alternatively, separate spectrometers can be utilized to control and acquire data from the separate modules within probe.
  • the location of box allows each circuit to be tuned independently outside of the magnet, which conserves space.
  • the box is coupled through connections to other standard components of the spectrometer including high-power amplifiers, a pre-amplifier, and a receiver (acquisition device).
  • Gas lines are also coupled to the probe. These lines provide the drive and bearing gas for the sample holders within the MAS modules. Additional gas lines can be utilized to provide each spinning module with separate drive and bearing gas.
  • each MAS module includes its own air supply lines, radio- frequency connections, and magic-angle adjustment mechanism, although some or all of these features may be combined.
  • Each spinning module may have variable-temperature capability, independent spinning speed control, and independent shimming parameters.
  • the NMR line with was investigated as a function of distance from the homogeneous region of the magnet.
  • the data was acquired on a CMX-II NMR spectrometer using a probe equipped with a 7.0 mm MAS (Revolution NMR).
  • the magnetic field strength was 7.05 Tesla.
  • FIG. 3 the magnetic field homogeneity for adamantane remained relatively unchanged as the sample was moved over a distance of approximately one centimeter in the magnet. This distance corresponds to a relatively large region over which a high-resolution MAS NMR spectrum could be acquired. This indicates that over this distance it may be possible to place two (or more) MAS systems in which both of them are in the homogeneous region of the magnetic field.

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  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Epidemiology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Magnetic Resonance Imaging Apparatus (AREA)

Abstract

L'invention a trait à une sonde de résonance magnétique nucléaire à l'état solide destinée à être utilisée dans un champ magnétique ayant une pluralité de modules de rotation à l'angle magique isolés positionnés à l'intérieur du logement. Le logement est configuré de sorte que la pluralité de modules de rotation à l'angle magique se trouvent dans une position stationnaire à l'intérieur d'une région homogène dudit champ magnétique pendant l'utilisation.
PCT/US2008/050905 2007-01-11 2008-01-11 Systèmes à haut rendement pour résonance magnétique nucléaire avec rotation à l'angle magique WO2008086525A2 (fr)

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US87988507P 2007-01-11 2007-01-11
US60/879,885 2007-01-11

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WO2008086525A3 WO2008086525A3 (fr) 2008-10-09

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US9500671B2 (en) 2011-10-10 2016-11-22 Purdue Research Foundation AFM-coupled microscale radiofrequency probe for magnetic resonance imaging and spectroscopy
WO2013055823A1 (fr) * 2011-10-10 2013-04-18 Purdue Research Foundation Sonde radiofréquence micro-échelle couplée par microscopie à force atomique (afm) pour spectroscopie et imagerie à résonance magnétique
US9995801B2 (en) * 2014-12-02 2018-06-12 University Of Kentucky Research Foundation Static multiple-sample NMR probe
DE102015222935B3 (de) * 2015-11-20 2017-03-09 Bruker Biospin Ag Winkelverstellbarer Messkopf einer NMR-MAS-Apparatur
JP7158966B2 (ja) * 2018-09-14 2022-10-24 株式会社東芝 ダイヤモンド基板、量子デバイス、量子システム、及び、ダイヤモンド基板の製造方法

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US6794874B2 (en) * 2001-09-27 2004-09-21 Jeol Ltd. Multiple tuning circuit and probe having multiple tuning circuit for NMR spectrometer
US20040222796A1 (en) * 2003-02-04 2004-11-11 Munson Eric Jon Solid-state nuclear magnetic resonance probe
US20060192559A1 (en) * 2000-11-03 2006-08-31 Ardenkjaer-Larsen Jan H Methods and devices for polarized NMR samples

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US4654592A (en) * 1985-01-14 1987-03-31 Varian Associates, Inc. Concurrent NMR analysis of multiple samples
WO2000050924A1 (fr) * 1999-02-26 2000-08-31 Purdue Research Foundation Analyse de multiples echantillons par resonance magnetique nucleaire
US7282919B2 (en) * 2005-02-10 2007-10-16 Doty Scientific, Inc. NMR CryoMAS probe for high-field wide-bore magnets

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US20060192559A1 (en) * 2000-11-03 2006-08-31 Ardenkjaer-Larsen Jan H Methods and devices for polarized NMR samples
US6794874B2 (en) * 2001-09-27 2004-09-21 Jeol Ltd. Multiple tuning circuit and probe having multiple tuning circuit for NMR spectrometer
US20040222796A1 (en) * 2003-02-04 2004-11-11 Munson Eric Jon Solid-state nuclear magnetic resonance probe

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WO2008086525A3 (fr) 2008-10-09
US20080169814A1 (en) 2008-07-17

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